US7875306B2 - Completely-soluble solid particle(s) based on dietary fibre(s) - Google Patents

Completely-soluble solid particle(s) based on dietary fibre(s) Download PDF

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Publication number
US7875306B2
US7875306B2 US11/573,216 US57321605A US7875306B2 US 7875306 B2 US7875306 B2 US 7875306B2 US 57321605 A US57321605 A US 57321605A US 7875306 B2 US7875306 B2 US 7875306B2
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Prior art keywords
hydrophobic
aroma
water
dietary fibres
solid
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US20080138492A1 (en
Inventor
Dominique Cingotti
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SINE SILEO
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Maya Flowers SA
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Classifications

    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/20Reducing nutritive value; Dietetic products with reduced nutritive value
    • A23L33/21Addition of substantially indigestible substances, e.g. dietary fibres
    • A23L33/22Comminuted fibrous parts of plants, e.g. bagasse or pulp
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/10Natural spices, flavouring agents or condiments; Extracts thereof
    • A23L27/12Natural spices, flavouring agents or condiments; Extracts thereof from fruit, e.g. essential oils
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/70Fixation, conservation, or encapsulation of flavouring agents
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/244Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from corms, tubers or roots, e.g. glucomannan
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/25Exudates, e.g. gum arabic, gum acacia, gum karaya or tragacanth
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/20Agglomerating; Granulating; Tabletting
    • A23P10/25Agglomeration or granulation by extrusion or by pressing, e.g. through small holes, through sieves or between surfaces
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/30Encapsulation of particles, e.g. foodstuff additives

Definitions

  • the invention relates to a completely-soluble solid particle based on soluble dietary fibre(s) and at least one active substance particularly for a dietetic, cosmetic or pharmaceutical purpose.
  • the particles of the invention may comprise any type of active substance, and preferably substances of plant origin, particularly in the form of a plant extract or part of a plant.
  • aromas as the active substance.
  • “aroma” here means any product or substance designed to be added to foods to give them an odour, a taste, or both.
  • aromas a distinction is made between natural aromatizing substances, aromatizing substances identical to natural aromatizing substances, artificial aromatizing substances, aromatizing preparations, processed aromas and smoke aromas.
  • a natural aromatizing substance is a chemically defined substance which is obtained either by appropriate physical methods, including distillation and solvent extraction, or by enzymatic or microbiological methods, from a material of plant or animal origin, taken as such or after its processing for human consumption by conventional food preparation methods, including drying, roasting and fermentation.
  • This category particularly includes essential oils and pure aromas.
  • An aromatizing substance identical to a natural aromatizing substance is a defined chemical substance which is chemically identical to a natural aromatizing substance after having been obtained by chemical synthesis or isolated by chemical methods.
  • An artificial aromatizing substance is a defined chemical substance which, having been obtained by chemical synthesis, is not chemically identical to a natural aromatizing substance.
  • An aromatizing preparation is a product, other than a natural aromatizing substance, concentrated or not, which is obtained by appropriate physical methods, including distillation and solvent extraction, or by enzymatic or microbiological methods, from a material of plant or animal origin, taken as such or after its processing for human consumption by conventional food preparation methods, including drying, roasting and fermentation.
  • a processed aroma is a product obtained by heating to a temperature not exceeding 180° C. for a period not exceeding 15 minutes of a mixture of ingredients which have aromatizing properties or not, provided that the components of the mixture comprise at east one ingredient containing nitrogen and at least one ingredient serving as a reducing sugar.
  • a smoke aroma is a smoke extract which is used in conventional food smoking methods.
  • soluble dietary fibres means any compound of completely-water-soluble plant cells, withstanding the various enzymatic hydrolyses occurring during a physiological process of digestion. More precisely, the enzymes of the organism abundantly present in the small intestine, such as sucrase-maltase, have no hydrolytic action on the bonds of the units forming the fibres, thereby causing no increase in glycemia, and in the rate of insulin in the blood. These fibres are composed of cellulose, hemicellulose, oligosaccharides, pectin, gums, waxes, these various compounds are those taken into account in the analyses of dietary fibres. Soluble fibres should be distinguished from sugars or sugar derivatives, such as for example sucrose, glucose, lactose, maltodextrin, etc., which are rapid or slow directly assimilable sugars.
  • the dietary fibres consist of a completely-water-soluble polymer selected particularly from the group comprising inulin, oligofructoses (also called fructo-oligosaccharides (FOS)), gum arabic, used alone or in mixtures.
  • inulin also called fructo-oligosaccharides (FOS)
  • FOS fructo-oligosaccharides
  • inulin is a mixture of oligomers and polymers of fructose, obtained by extraction particularly from chicory roots.
  • the structure of inulin can be represented by the formula GFn, in which:
  • inulin consists of some 60 fructose units.
  • Fructo-oligosaccharides correspond to a mixture of oligomers and polymers of fructose obtained by inulin hydrolysis.
  • the FOS structure can be represented by the formula GFn or Fm, in which:
  • FOS consist of 10 fructose units.
  • Document WO 99/06028 describes a method for producing granules from dietary fibres like those of the present invention. More precisely, the dietary fibres are in atomized form and are contacted with an extract of active ingredient, for example essential oils, in a solvent medium and in the absence of binder, before a final oven drying step, to remove the solvent.
  • an extract of active ingredient for example essential oils
  • a porous atomized support with a high specific surface area is used, in order to impregnate the maximum of extract at the surface and in the pores of the structure.
  • the absence of binder makes it possible to recover, at the end of the method, as many atomized particles as existed initially.
  • the solvent must be selected so that it is incapable of solubilizing the dietary fibres.
  • the structure of the dietary fibres is unchanged during the method.
  • the granules obtained, 1 mm in size have mechanical properties, particularly hardness, incompatible with a subsequent calibration operation. In fact, the granules cannot be reduced in size without causing a high loss of material, due to their high friability.
  • the problem which the invention proposes to solve is hence to develop a method for preparing completely-soluble granules, based particularly on aromas, in which the aromatic profile of the said aromas is unchanged from the original profile.
  • the objective is to have granules which are then suitable for calibration and conditioning without loss of material.
  • the Applicant has developed a novel method essentially consisting in extruding in a die, without the addition of water, a mixture comprising soluble dietary fibres and at least one active substance.
  • the Applicant has in fact found that the dietary fibres selected from the abovementioned group, solid at ambient temperature, are converted to become semi-solid under the effect of heat, and in the absence of solvent and, in general, of any additive. Furthermore, it has been observed that this change of state occurred from a temperature of about 30° C. or more, suitable for preparing particles based on heat-sensitive active ingredients. Finally, the solid state recovered after cooling has a much higher hardness and lower friability compared to the corresponding values of the dietary fibres in the natural state.
  • the dietary fibres constitute an ideal support for the production of completely-soluble particles for ingestion, making it possible, thanks to the change of state caused by the temperature rise alone, on the one hand, to overcome the need for the presence of water mentioned in document WO 01/17372 and on the other, to include heat-sensitive active ingredients in a matrix and not impregnate them on individualized particles as is the case in document WO 99/06028.
  • the advantage of this method is hence to restore all the properties of the starting active ingredient and particularly its analytical profile.
  • the hardened form obtained after cooling has a high hardness suitable for calibrating the particles in a wide range and as required, and without any problem of friability.
  • the hardness of the particle depends on the type of active substance incorporated. If the active substance is mixed with the dietary fibres in liquid form, the particle will then, in the abovementioned range, have a lower hardness than if the active substance is incorporated in solid form. The hardness will also be influenced by the content of the active substance in the particle. In practice, the active substance accounts for between 0.1 and 10% by weight of the particle.
  • the support contains soluble dietary fibres.
  • the support consists exclusively of soluble dietary fibres.
  • the active substance is advantageously an aroma.
  • the particle contains, in addition to the dietary fibres, between 2 and 5% by weight of essential oil, and has a hardness of between 0.2 and 0.3 GPa.
  • the particles obtained can be used in various galenic forms, such as particularly sachet, tablet, capsule, powder, inclusion in pasty forms, etc.
  • Such a particle can be obtained by a method in which, in the absence of hydrophilic solvent:
  • the method is carried out in the absence of a hydrophilic solvent to thereby avoid solubilization of the dietary fibres.
  • hydrophilic solvent therefore means any solvent capable of dissolving the dietary fibres, particularly water.
  • the dietary fibres are used in powder form.
  • the powder form may correspond to an atomized or micronized form from natural fibres.
  • the specific surface area atomized, micronized is immaterial insofar as the material undergoes a change of state causing the particles to lose their basic structure.
  • the fibres are mixed to obtain a semi-solid mass.
  • the active substance used, but also on the mechanical properties of the extruder, the latter generates heat during its operation, that is, in the absence of an external energy input.
  • the temperature may vary throughout the method within the range of values comprised between 30 and 130° C., with the understanding that a person skilled in the art will adjust the operating parameters of the extruder to avoid reaching temperatures capable of distorting the analytical profile of the active ingredient.
  • the active substance can be incorporated with the fibres during the temperature rise or once the semi-solid state has been reached.
  • the active material can be incorporated in various forms which depend on the physicochemical nature of the said active substance.
  • the active substance When the active substance is in solid form, it is incorporated either directly or in dissolved or dispersed form in a hydrophobic solvent, with the understanding that any hydrophilic solvent is, as already stated, prohibited. Thus in all cases in which the active ingredient is water-soluble, it is placed in a hydrophobic medium by any technique known to a person skilled in the art before being contacted with the dietary fibres.
  • the hydrophobic solvent is liquid at ambient temperature. It is particularly selected from the group comprising triacetin, vegetable or mineral oils, without this list being limiting.
  • the active substance When the active substance is liquid in the natural state, it can be incorporated as such, particularly by granulation in the dietary fibres provided that it is hydrophobic. If not, the liquid active substance is made hydrophobic prior to its mixing with the dietary fibres.
  • a third step the mixture of dietary fibres in which the active substance is included is extruded. This extrusion is carried out through a die, while the mixture is still in the semi-solid state.
  • the filaments cool in contact with the ambient temperature.
  • the size of the die is obviously selected according to the desired size of the particles, with the understanding that the filaments obtained are then divided.
  • This final division step can be carried out by various methods such as grinding or even crushing.
  • FIG. 1 corresponds to the gas chromatographic profiles respectively of a natural orange aroma ( FIG. 1 a ) and the same aroma incorporated in a particle of the invention ( FIG. 1 b ).
  • FIG. 2 corresponds to the curve obtained after the indentation test performed by the dynamic method on an elastoplastic material: silica.
  • FIGS. 3 , 4 and 5 correspond to the curves obtained after an indentation test carried out by the dynamic method respectively on epoxy ( FIGS. 3 a, b, c ), particles of the invention having a size of 1 mm ( FIGS. 4 a, b, c ) and 2 mm ( FIGS. 5 a, b, c ).
  • an inulin/FOS mixture is introduced in a ratio 60/40 (Raftiline raftilose® P95 from ORAFTI or Fibrulose® from COSUCRA) in powder form and essential oil of orange in a weight ratio of 96/4.
  • the mixture of the two products generates a temperature rise to about 35° C., at which temperature the mixture becomes semi-solid.
  • the said mixture is then extruded through the die and the filaments formed are calibrated to a size of 4 mm. After cooling, the particles formed are recovered.
  • Gas chromatography is then carried out to compare the profile of the reference essential oil and that of the essential oil recovered after dissolution of the particle in water and distillation of the water.
  • FIGS. 1 a and 1 b show the gas chromatography profiles of a reference (essential oil of orange) ( FIG. 1 ) and of the sample ( FIG. 1 b ).
  • an inulin/FOS mixture is introduced in a ratio 60/40 (Raftiline raftilose® P95 from ORAFTI or Fibrulose® from COSUCRA) in powder form and essential oil of mint in a weight ratio of 97/3.
  • the mixture of the two products generates a temperature rise to about 35° C., at which temperature the mixture becomes semi-solid.
  • the said mixture is then extruded through the die and the filaments are then calibrated. After cooling, particles are recovered having an average size of between 0.335 and 2.25 mm.
  • the hardness of the particles obtained is measured by a nanoindentation on an XP® nanoindenter from Nano Instruments.
  • the test method used is a dynamic method.
  • the principle of the dynamic method is based on the superimposition of a continuous movement and an oscillating movement at fixed frequency (32 Hz) and low amplitude (5 mm).
  • loading is accompanied by a succession of small loadings and small unloadings, which means that the material is elastically and then plastically and then again elastically deformed.
  • the tests are performed at a constant loading rate P′/P (3.10 ⁇ 2 s ⁇ 1 ).
  • the curve shown in FIG. 2 corresponds to the indentation test performed by the dynamic method on an elastoplastic material: silica.
  • D ⁇ contact damping, phase difference between the displacement and the force measured using the synchronous detector.
  • FIGS. 3 a,b,c , 4 a,b,c and 5 a,b,c show the results obtained by nanoindentation using a Berkovich indenter on a reference (epoxy matrix) and particles having a size of 1 mm ( FIG. 4 ) and 2 mm ( FIG. 5 ), under a load of 10 mN.
  • the hardness measured both for the 1 mm grains and for the 2 mm grains is between 0.25 and 0.28 GPa.

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Dispersion Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
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  • Coloring Foods And Improving Nutritive Qualities (AREA)
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US11/573,216 2004-08-06 2005-08-01 Completely-soluble solid particle(s) based on dietary fibre(s) Active 2026-12-17 US7875306B2 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR0451807A FR2873896B1 (fr) 2004-08-06 2004-08-06 Particule(s) solides(s) soluble(s) a base de fibre(s) alimentaire(s)
FR0451807 2004-08-06
PCT/FR2005/050636 WO2006021720A1 (fr) 2004-08-06 2005-08-01 Particule(s) solide(s) entierement soluble(s) a base de fibre(s) alimentaire(s)

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US20080138492A1 US20080138492A1 (en) 2008-06-12
US7875306B2 true US7875306B2 (en) 2011-01-25

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US (1) US7875306B2 (de)
EP (1) EP1773135B1 (de)
ES (1) ES2748464T3 (de)
FR (1) FR2873896B1 (de)
WO (1) WO2006021720A1 (de)

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EP1773135B1 (de) 2019-07-24
FR2873896B1 (fr) 2007-06-01
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US20080138492A1 (en) 2008-06-12
FR2873896A1 (fr) 2006-02-10
EP1773135A1 (de) 2007-04-18

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